DIN EN 13999-2-2014 en 5831 Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 2 Determination of.pdf

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1、March 2014 Translation by DIN-Sprachendienst.English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、83.180!%,/“2099312www.din.deDDIN EN 13999-2Adhesives Short term method for measuring the emission properties of low-solventor solvent-free adhesives after application Part 2: Determination of volatile organic compounds;English version EN 13999-2:2013,English translation of DIN EN 13999-2:2014-03Kleb

3、stoffe Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lsemittelarmen oderlsemittelfreien Klebstoffen nach der Applikation Teil 2: Bestimmung flchtiger organischer Verbindungen;Englische Fassung EN 13999-2:2013,Englische bersetzung von DIN EN 13999-2:2014-03Adhsifs Mthode de mesurage ra

4、pide des caractristiques missives des adhsifs teneur faibleou nulle en solvants aprs application Partie 2: Dosage des composs organiques volatils;Version anglaise EN 13999-2:2013,Traduction anglaise de DIN EN 13999-2:2014-03SupersedesDIN EN 13999-2:2007-07www.beuth.deDocument comprises 15 pagesIn ca

5、se of doubt, the German-language original shall be considered authoritative.02.14DIN EN 13999-2:2014-03 2 A comma is used as the decimal marker. National foreword This document (EN 13999-2:2013) has been prepared by Technical Committee CEN/TC 193 “Adhesives” (Secretariat: AENOR, Spain). The responsi

6、ble German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-04-06 AA Klebstoffe Terminologie; physikalisch-chemische Prfungen. The DIN Standard corresponding to the International Standard referred to in Clause 2 of this sta

7、ndard is as follows: ISO 16000-6 DIN ISO 16000-6 Amendments This standard differs from DIN EN 13999-2:2007-07 as follows: a) the foreword now includes a “Safety Statement” and an “Environmental Statement”; b) new definitions have been included for VVOC, VOC and SVOC; c) the note relating to the prep

8、aration of sampling tubes has been revised (Subclause 6.1); d) the preconditioning temperature of the sampling tubes has been changed from (300 10) C to (320 10) C (Subclause 6.1.2); e) acceptance criteria for the tube blank during conditioning have been revised (Subclause 6.1.2); f) the recommended

9、 sampling flow rate for the test chamber air sampling has been revised (Subclause 6.1.2); g) the time to desorb and analyse the volatile organic compounds has been changed from within 4 weeks to preferably within 2 weeks, but not later than 4 weeks (Subclause 6.7.1); h) the desorption temperature ha

10、s been changed from 260 C up to 280 C to 200 C up to 320 C (Subclause 6.7.2); i) normative references have been updated; j) the standard has been editorially revised. Previous editions DIN V ENV 13999-2: 2003-02 DIN EN 13999-2: 2007-07 National Annex NA (informative) Bibliography DIN ISO 16000-6, In

11、door air Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromatography using MS/FID EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13999-2 December 2013 ICS 83.180 Supersedes EN 13999-2:2007E

12、nglish Version Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 2: Determination of volatile organic compoundsAdhsifs - Mthode de mesurage rapide des caractristiques missives des adhsifs teneur faible ou nulle en so

13、lvants aprs application - Partie 2: Dosage des composs organiques volatils Klebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lsemittelarmen oder lsemittelfreien Klebstoffen nach der Applikation - Teil 2: Bestimmung flchtiger organischer Verbindungen This European Standard was

14、 approved by CEN on 19 October 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such na

15、tional standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own lan

16、guage and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greec

17、e, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG C

18、EN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13999-2:2013: EEN 13999-2:2013 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Principle 4 4 R

19、eagents and materials 4 5 Apparatus .5 6 Procedure .6 7 Identification and calculation .9 8 Precision and bias 11 9 Test report . 11 10 Quality control . 11 Bibliography . 13 DIN EN 13999-2:2014-03 EN 13999-2:2013 (E) 3 Foreword This document (EN 13999-2:2013) has been prepared by Technical Committe

20、e CEN/TC 193 “Adhesives”, the secretariat of which is held by AENOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2014, and conflicting national standards shall be withdrawn at the latest

21、by June 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 13999-2:2007. EN 13999-2:2013 includes the f

22、ollowing significant technical changes with respect to EN 13999-2:2007: a) change in the calculation of total VOC; b) harmonization of the testing conditions to EN ISO 16000-9. EN 13999, under the general title Adhesives Short -term method for measuring the emission properties of low-solvent or solv

23、ent-free adhesives after application, consists of the following parts: Part 1: General procedure Part 2: Determination of volatile organic compounds Part 3: Determination of volatile aldehydes Part 4: Determination of volatile diisocyanates SAFETY STATEMENT Persons using this document should be fami

24、liar with the normal laboratory practice, if applicable. This document does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory condi

25、tions. ENVIRONMENTAL STATEMENT It is understood that some of the material permitted in this European Standard may have negative environmental impact. As technological advantages lead to acceptable alternatives for these materials, they will be eliminated from this European Standard to the extent pos

26、sible. At the end of the test, the user of this European Standard should take care to carry out an appropriate disposal of the wastes, according to local regulation. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implem

27、ent this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,

28、Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 13999-2:2014-03 EN 13999-2:2013 (E) 4 1 Scope This European Standard specifies a method for the determination of single volatile organic compounds (VOC) and of the total amount of volatile organic compounds (TVOCEN

29、13999) in the exhaust air of an emission test chamber after application of a low-solvent or solvent-free adhesive as defined in EN 923:2005+A1:2008. The method is based on use of a solid sorbent with subsequent desorption and gas chromatographic analysis. The method is applicable to measurement of n

30、on-polar and slightly polar VOC. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referen

31、ced document (including any amendments) applies. EN 1232, Workplace atmospheres - Pumps for personal sampling of chemical agents - Requirements and test methods EN 13999-1, Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application

32、- Part 1: General procedure EN ISO 16000-9, Indoor air - Part 9: Determination of the emission of volatile organic compounds from building products and furnishing - Emission test chamber method (ISO 16000-9) EN ISO 16017-1, Indoor, ambient and workplace air - Sampling and analysis of volatile organi

33、c compounds by sorbent tube/thermal desorption/capillary gas chromatography - Part 1: Pumped sampling (ISO 16017-1) ISO 16000-6, Indoor air - Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption and gas chromato

34、graphy using MS or MS-FID 3 Principle A sufficient volume of test chamber air is drawn with an appropriate flow through a sorbent tube (or several tubes in series) containing a solid sorbent. Volatile organic compounds (VOC) are retained by the sorbent tube, which is subsequently analysed in the lab

35、oratory. The VOC are desorbed from the sampling tube and transferred by a flow of inert carrier gas into a capillary gas chromatograph coupled to a mass spectrometric detector (MS) and to a flame ionisation detector (FID) or only to a mass spectrometric detector. 4 Reagents and materials 4.1 Volatil

36、e organic compounds for calibration Compounds of gas chromatographic grade. 4.2 Methanol Methanol of gas chromatographic grade. DIN EN 13999-2:2014-03 EN 13999-2:2013 (E) 5 4.3 Sorbent material For general purpose, poly(2,6-diphenyl-p-phenylene oxide, particle size (0,18 to 0,25) mm i.e. (60 to 80)

37、mesh (Tenax1)TA 1 or equivalent sorbent materials) shall be used. For the determination of very volatile carcinogenic organic compounds (e.g. vinyl chloride), Carbopack X 1)or equivalent sorbent materials as described in EN ISO 16017-1 shall be used. 4.4 Carrier gas Helium, argon or nitrogen with a

38、purity 99,999 % or better. 5 Apparatus 5.1 Sorbent tubes Sorbent tubes made from stainless steel or glass that can be filled with at least 200 mg of Tenax TA sorbent (4.3) are used. For example, tubes with 6 mm external diameter, 5 mm internal diameter and 90 mm long fulfil the requirement and are u

39、sed in many commercial thermal desorbing devices. It is recommended to use unsilanised glass wool or other suitable mechanism, e.g. stainless steel frit to retain the sorbent in the tube and metal screw caps and polytetrafluoroethylene (PTFE) ferrules for closing the sorbent tube. Carbopack X (4.3)

40、or equivalent tubes are filled as described in EN ISO 16017-1. 5.2 Sorbent tube unions Two sorbent tubes may be connected in series during sampling with metal screw cap couplings with PTFE ferrules. 5.3 Syringes A precision 10 l liquid syringe readable to 0,1 l. 5.4 Sampling pump The pump shall fulf

41、il the requirements of EN 1232 or equivalent. 5.5 Tubing PE poly(ethylene) or PTFE tubing of appropriate diameter to ensure a leak-proof fit to both pump and sample tube. Sampling tubes shall not be used with plastic tubing other than PTFE upstream of the sorbent to avoid interference from contamina

42、nts. 5.6 Flow meter calibrator Bubble meter or other appropriate suitable device for gas flow calibration. 5.7 Gas chromatograph A capillary gas chromatograph coupled to a mass spectrometric detector and to a flame ionisation detector or only to a mass spectrometric detector shall be used in accorda

43、nce with EN ISO 16017-1 and ISO 16000-6. 1) Carbopack X and Tenax TA are examples of suitable products available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. DIN EN 13999-2:2014-03 EN 139

44、99-2:2013 (E) 6 5.8 Thermal desorption apparatus Apparatus for two-stage thermal desorption of sorbent tubes and transfer of desorbed vapours via an inert gas flow into a gas chromatograph is required. A typical apparatus contains a mechanism for holding the tubes to be desorbed whilst they are heat

45、ed and purged simultaneously with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas flow rate. The apparatus may also incorporate additional features, such as automatic sample tube loading, leak testing, and a cold trap or another suitable device to concentr

46、ate the desorbed sample. The desorbed sample, contained in the purge gas, is routed to the gas chromatograph and capillary column via a heated transfer line. 5.9 Injection facility for preparing standards by liquid spiking Use a commercially available unit for preparation of calibration standards or

47、 any other device allowing reproducible preparation of calibration standards. 5.10 Emission test chamber An emission test chamber as described in EN 13999-1 or in EN ISO 16000-9 shall be used. 6 Procedure 6.1 Preparation of sampling tubes 6.1.1 Preconditioning Use commercially pre-cleaned sampling t

48、ubes containing Tenax TA or sampling tubes that are preconditioned and filled in the laboratory as described for Tenax TA in this clause. For special purposes such as determination of specific carcinogenic volatile organic compounds as foreseen in EN 13999-1, other sorbent materials as described in

49、EN ISO 16017-1 can be taken. Remove trace impurities of manufactured Tenax TA before using it for VOC sampling. The success of the cleaning procedure is checked by performing analysis of the blank sorbent. Tube blanks are acceptable if no individual interfering artefact peaks exceed 2 ng and if TVOC levels do not exceed 20 ng after subtraction of non-interfering VOC artefacts. NOTE Usually keeping the tubes at a temperature of (320 10) C for at least 3 h using carrier gas flow of 50 ml/min to 100 ml/min is